Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805037864/bh6045sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805037864/bh6045Isup2.hkl |
CCDC reference: 294047
Data collection: RAPID-AUTO (Rigaku, 1998; cell refinement: PROCESS-AUTO (Rigaku/MSC, 2005); data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: CrystalStructure (Rigaku/MSC, 2005).
[Pd(C5H4N5)(C9H11N2O)]·3.5H2O | F(000) = 1896.00 |
Mr = 466.81#933.61 | Dx = 1.759 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.7107 Å |
Hall symbol: -C 2yc | Cell parameters from 14802 reflections |
a = 23.75 (2) Å | θ = 3.1–27.5° |
b = 6.869 (5) Å | µ = 1.09 mm−1 |
c = 21.65 (2) Å | T = 123 K |
β = 93.46 (3)° | Plate, brown |
V = 3526 (5) Å3 | 0.50 × 0.15 × 0.05 mm |
Z = 8#4 |
Rigaku R-AXIS RAPID diffractometer | 3440 reflections with F2 > 2σ(F2) |
Detector resolution: 10.00 pixels mm-1 | Rint = 0.014 |
ω scans | θmax = 27.5° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −30→30 |
Tmin = 0.682, Tmax = 0.947 | k = −8→8 |
17133 measured reflections | l = −28→28 |
4009 independent reflections |
Refinement on F2 | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.026 | w = 1/[σ2(Fo2) + (0.0397P)2 + 7.5219P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.070 | (Δ/σ)max = 0.001 |
S = 1.07 | Δρmax = 1.61 e Å−3 |
4009 reflections | Δρmin = −0.70 e Å−3 |
283 parameters |
Geometry. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 3.6253 (0.0160) x + 6.7558 (0.0066) y + 2.2919 (0.0142) z = 5.7581 (0.0073) * -0.0617 (0.0009) O11 * 0.0664 (0.0009) N11 * -0.0635 (0.0009) N12 * 0.0601 (0.0008) N9 * -0.0012 (0.0007) Pd1 Rms deviation of fitted atoms = 0.0563 - 5.6843 (0.0157) x + 6.5880 (0.0065) y + 3.5790 (0.0102) z = 4.9557 (0.0076) * -0.0112 (0.0013) O11 * 0.0022 (0.0018) C11 * 0.0058 (0.0018) C12 * 0.0041 (0.0020) C13 * -0.0073 (0.0019) C14 * -0.0042 (0.0019) C15 * 0.0095 (0.0019) C16 * -0.0030 (0.0017) C17 * 0.0041 (0.0014) N11 Rms deviation of fitted atoms = 0.0064 - 0.7008 (0.0138) x + 6.7555 (0.0066) y + 3.8993 (0.0108) z = 6.3425 (0.0064) Angle to previous plane (with approximate e.s.d.) = 12.23 (0.06) * -0.0026 (0.0019) N1 * -0.0112 (0.0018) C2 * 0.0054 (0.0016) N3 * 0.0019 (0.0018) C4 * -0.0143 (0.0021) C5 * 0.0021 (0.0022) C6 * 0.0189 (0.0017) N6 * -0.0202 (0.0017) N7 * 0.0041 (0.0017) C8 * 0.0160 (0.0016) N9 Rms deviation of fitted atoms = 0.0119 |
Refinement. Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt). |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Pd1 | 0.25429 (1) | 0.98544 (2) | 0.00928 (1) | 0.01462 (7) | |
O1 | 0.50434 (7) | 0.8580 (3) | 0.04621 (9) | 0.0350 (4) | |
O2 | 0.4661 (1) | 0.8657 (6) | 0.1651 (1) | 0.087 (1) | |
O4 | 0.5000 | 0.1467 (5) | 0.2500 | 0.0484 (7) | |
O11 | 0.23326 (7) | 0.9959 (2) | −0.08116 (8) | 0.0192 (3) | |
O31 | 0.4125 (3) | 0.5098 (9) | 0.1876 (3) | 0.073 (2) | 0.50 |
O32 | 0.4671 (4) | 0.598 (1) | 0.2417 (3) | 0.094 (2) | 0.50 |
N3 | 0.17065 (8) | 0.8790 (3) | 0.13579 (8) | 0.0203 (4) | |
N1 | 0.07644 (8) | 0.8479 (3) | 0.17071 (9) | 0.0276 (4) | |
N7 | 0.07604 (8) | 0.9425 (3) | 0.00216 (9) | 0.0220 (4) | |
N9 | 0.17133 (7) | 0.9448 (3) | 0.02463 (8) | 0.0166 (3) | |
N11 | 0.33443 (7) | 1.0419 (3) | −0.00092 (9) | 0.0172 (3) | |
N12 | 0.28155 (8) | 0.9601 (3) | 0.09999 (9) | 0.0230 (4) | |
N6 | −0.00477 (9) | 0.8806 (4) | 0.1049 (1) | 0.0388 (6) | |
C2 | 0.1334 (1) | 0.8484 (4) | 0.1778 (1) | 0.0244 (5) | |
C6 | 0.05216 (9) | 0.8791 (4) | 0.1134 (1) | 0.0255 (5) | |
C5 | 0.08752 (9) | 0.9086 (3) | 0.0645 (1) | 0.0203 (4) | |
C4 | 0.14549 (9) | 0.9089 (3) | 0.0786 (1) | 0.0165 (4) | |
C8 | 0.12757 (9) | 0.9634 (3) | −0.0185 (1) | 0.0190 (4) | |
C11 | 0.26814 (9) | 1.0509 (3) | −0.1234 (1) | 0.0185 (4) | |
C12 | 0.2452 (1) | 1.0651 (3) | −0.1848 (1) | 0.0233 (4) | |
C13 | 0.2776 (1) | 1.1187 (4) | −0.2326 (1) | 0.0289 (5) | |
C14 | 0.3349 (1) | 1.1606 (4) | −0.2218 (1) | 0.0295 (5) | |
C15 | 0.3585 (1) | 1.1490 (3) | −0.1621 (1) | 0.0254 (5) | |
C16 | 0.32635 (9) | 1.0961 (3) | −0.1120 (1) | 0.0185 (4) | |
C17 | 0.35623 (9) | 1.0874 (3) | −0.0520 (1) | 0.0189 (4) | |
C18 | 0.3707 (1) | 1.0288 (3) | 0.0569 (1) | 0.0216 (4) | |
C19 | 0.33455 (9) | 1.0722 (4) | 0.1099 (1) | 0.0246 (5) | |
H1 | 0.1485 | 0.8239 | 0.2177 | 0.029* | |
H2 | −0.0252 | 0.8618 | 0.1358 | 0.047* | |
H3 | −0.0205 | 0.9004 | 0.0687 | 0.047* | |
H4 | 0.1332 | 0.9891 | −0.0598 | 0.023* | |
H5 | 0.2072 | 1.0374 | −0.1933 | 0.028* | |
H6 | 0.2611 | 1.1272 | −0.2726 | 0.035* | |
H7 | 0.3568 | 1.1957 | −0.2542 | 0.035* | |
H8 | 0.3966 | 1.1768 | −0.1547 | 0.031* | |
H9 | 0.3945 | 1.1172 | −0.0501 | 0.023* | |
H10 | 0.4014 | 1.1220 | 0.0562 | 0.026* | |
H11 | 0.3868 | 0.8993 | 0.0614 | 0.026* | |
H12 | 0.3540 | 1.0347 | 0.1488 | 0.029* | |
H13 | 0.3264 | 1.2104 | 0.1114 | 0.029* | |
H14 | 0.2553 | 1.0068 | 0.1243 | 0.028* | |
H15 | 0.2877 | 0.8341 | 0.1096 | 0.028* | |
H21 | 0.4812 | 0.7533 | 0.0343 | 0.053* | |
H22 | 0.4900 | 0.8803 | 0.0852 | 0.053* | 0.56 |
H23 | 0.4973 | 0.9347 | 0.0103 | 0.053* | 0.44 |
H24 | 0.4905 | 0.9696 | 0.1783 | 0.131* | |
H25 | 0.4712 | 0.7948 | 0.2032 | 0.131* | 0.22 |
H26 | 0.4902 | 0.8176 | 0.1350 | 0.131* | 0.78 |
H27 | 0.4385 | 0.6149 | 0.1964 | 0.110* | 0.50 |
H28 | 0.4151 | 0.4613 | 0.2292 | 0.110* | 0.50 |
H29 | 0.4514 | 0.5494 | 0.2782 | 0.141* | 0.50 |
H30 | 0.4794 | 0.7196 | 0.2599 | 0.141* | 0.50 |
H31 | 0.5311 | 0.2268 | 0.2356 | 0.073* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pd1 | 0.01053 (9) | 0.01629 (9) | 0.0172 (1) | −0.00009 (5) | 0.00228 (6) | −0.00006 (6) |
O1 | 0.0187 (8) | 0.040 (1) | 0.047 (1) | −0.0026 (7) | 0.0015 (8) | −0.0108 (9) |
O2 | 0.076 (2) | 0.128 (3) | 0.060 (2) | −0.014 (2) | 0.021 (2) | −0.039 (2) |
O4 | 0.055 (2) | 0.049 (2) | 0.044 (2) | 0.0000 | 0.018 (1) | 0.0000 |
O11 | 0.0144 (7) | 0.0249 (8) | 0.0184 (8) | −0.0010 (5) | 0.0008 (6) | 0.0008 (6) |
O31 | 0.070 (4) | 0.099 (5) | 0.055 (3) | 0.030 (3) | 0.037 (3) | 0.023 (3) |
O32 | 0.133 (6) | 0.089 (5) | 0.066 (4) | −0.052 (4) | 0.051 (4) | −0.007 (4) |
N3 | 0.0189 (9) | 0.0210 (9) | 0.0214 (9) | 0.0018 (7) | 0.0042 (7) | 0.0001 (7) |
N1 | 0.022 (1) | 0.033 (1) | 0.029 (1) | 0.0031 (8) | 0.0101 (8) | 0.0080 (9) |
N7 | 0.0140 (8) | 0.0258 (9) | 0.026 (1) | −0.0008 (7) | 0.0021 (7) | 0.0032 (8) |
N9 | 0.0133 (8) | 0.0168 (8) | 0.0200 (9) | −0.0002 (7) | 0.0031 (7) | 0.0000 (7) |
N11 | 0.0133 (8) | 0.0172 (8) | 0.0212 (9) | 0.0004 (7) | 0.0012 (7) | −0.0024 (7) |
N12 | 0.0170 (9) | 0.033 (1) | 0.0189 (9) | −0.0022 (8) | 0.0007 (7) | 0.0028 (8) |
N6 | 0.017 (1) | 0.058 (2) | 0.043 (1) | 0.002 (1) | 0.0092 (9) | 0.024 (1) |
C2 | 0.023 (1) | 0.027 (1) | 0.024 (1) | 0.0023 (9) | 0.0047 (9) | 0.0029 (9) |
C6 | 0.018 (1) | 0.026 (1) | 0.033 (1) | 0.0018 (9) | 0.0080 (9) | 0.009 (1) |
C5 | 0.016 (1) | 0.019 (1) | 0.026 (1) | −0.0006 (8) | 0.0048 (8) | 0.0023 (9) |
C4 | 0.0156 (9) | 0.0132 (9) | 0.021 (1) | 0.0013 (7) | 0.0049 (8) | −0.0006 (8) |
C8 | 0.014 (1) | 0.020 (1) | 0.023 (1) | −0.0018 (8) | 0.0016 (8) | 0.0006 (8) |
C11 | 0.021 (1) | 0.0136 (9) | 0.021 (1) | 0.0031 (8) | 0.0043 (8) | −0.0018 (8) |
C12 | 0.025 (1) | 0.023 (1) | 0.022 (1) | 0.0016 (9) | 0.0015 (9) | −0.0028 (9) |
C13 | 0.037 (1) | 0.029 (1) | 0.021 (1) | 0.001 (1) | 0.005 (1) | −0.002 (1) |
C14 | 0.039 (1) | 0.029 (1) | 0.023 (1) | −0.005 (1) | 0.014 (1) | −0.0013 (9) |
C15 | 0.025 (1) | 0.024 (1) | 0.028 (1) | −0.0063 (9) | 0.0109 (9) | −0.0055 (9) |
C16 | 0.021 (1) | 0.0146 (9) | 0.021 (1) | −0.0009 (8) | 0.0060 (8) | −0.0031 (8) |
C17 | 0.0143 (9) | 0.017 (1) | 0.026 (1) | −0.0017 (8) | 0.0055 (8) | −0.0031 (8) |
C18 | 0.015 (1) | 0.025 (1) | 0.025 (1) | −0.0015 (8) | −0.0012 (9) | −0.0000 (9) |
C19 | 0.018 (1) | 0.032 (1) | 0.023 (1) | −0.0018 (9) | 0.0000 (8) | −0.002 (1) |
Pd1—O11 | 1.993 (2) | N11—C18 | 1.479 (3) |
Pd1—N9 | 2.037 (2) | N12—C19 | 1.480 (3) |
Pd1—N11 | 1.968 (2) | N12—H14 | 0.9000 |
Pd1—N12 | 2.038 (2) | N12—H15 | 0.9000 |
O1—H21 | 0.9322 | N6—C6 | 1.353 (3) |
O1—H22 | 0.9423 | N6—H2 | 0.8603 |
O1—H23 | 0.9461 | N6—H3 | 0.8600 |
O2—H24 | 0.9537 | C2—H1 | 0.9301 |
O2—H25 | 0.9582 | C6—C5 | 1.404 (3) |
O2—H26 | 0.9528 | C5—C4 | 1.392 (3) |
O4—H31 | 0.9861 | C8—H4 | 0.9301 |
O4—H31 | 0.9861 | C11—C12 | 1.410 (3) |
O11—C11 | 1.325 (3) | C11—C16 | 1.423 (3) |
O31—H27 | 0.9614 | C12—C13 | 1.376 (3) |
O31—H28 | 0.9590 | C12—H5 | 0.9301 |
O32—O32 | 1.58 (1) | C13—C14 | 1.398 (4) |
O32—H27 | 1.1646 | C13—H6 | 0.9300 |
O32—H29 | 0.9551 | C14—C15 | 1.378 (3) |
O32—H30 | 0.9601 | C14—H7 | 0.9301 |
N3—C2 | 1.323 (3) | C15—C16 | 1.412 (3) |
N3—C4 | 1.357 (3) | C15—H8 | 0.9300 |
N1—C2 | 1.352 (3) | C16—C17 | 1.443 (3) |
N1—C6 | 1.354 (3) | C17—H9 | 0.9299 |
N7—C5 | 1.381 (3) | C18—C19 | 1.505 (3) |
N7—C8 | 1.335 (3) | C18—H10 | 0.9700 |
N9—C4 | 1.375 (3) | C18—H11 | 0.9700 |
N9—C8 | 1.360 (3) | C19—H12 | 0.9700 |
N11—C17 | 1.288 (3) | C19—H13 | 0.9700 |
Pd1···Pd1 | 3.2642 (2) | C5···H11 | 3.5320 |
Pd1···N3 | 3.555 (2) | C5···H21 | 3.4947 |
Pd1···N9 | 3.542 (2) | C5···H21 | 2.8383 |
Pd1···C4 | 3.110 (2) | C5···H23 | 3.4419 |
Pd1···C8 | 3.036 (2) | C4···N11 | 3.570 (3) |
Pd1···C11 | 2.945 (2) | C4···C8 | 2.153 (3) |
Pd1···C16 | 3.308 (2) | C4···C15 | 3.539 (3) |
Pd1···C17 | 2.915 (2) | C4···C16 | 3.597 (3) |
Pd1···C18 | 2.907 (2) | C4···C16 | 3.532 (3) |
Pd1···C19 | 2.869 (2) | C4···C17 | 3.457 (3) |
Pd1···H4 | 3.1601 | C4···C17 | 3.508 (3) |
Pd1···H11 | 3.3299 | C4···H1 | 3.0637 |
Pd1···H13 | 3.1231 | C4···H4 | 3.0446 |
Pd1···H14 | 2.4941 | C4···H8 | 3.4663 |
Pd1···H15 | 2.4942 | C4···H9 | 3.4370 |
Pd1···H15 | 3.4825 | C4···H14 | 2.8135 |
O1···O1 | 2.793 (3) | C4···H15 | 3.4407 |
O1···O2 | 2.783 (4) | C8···N11 | 3.535 (3) |
O1···N7 | 3.486 (3) | C8···N6 | 3.535 (3) |
O1···N7 | 2.960 (3) | C8···C17 | 3.454 (3) |
O1···N6 | 3.529 (3) | C8···C18 | 3.482 (3) |
O1···C17 | 3.327 (3) | C8···C18 | 3.587 (3) |
O1···C18 | 3.403 (3) | C8···H3 | 2.8608 |
O1···H3 | 3.2407 | C8···H9 | 3.2974 |
O1···H3 | 3.0981 | C8···H10 | 3.0302 |
O1···H8 | 3.2308 | C8···H11 | 2.6730 |
O1···H9 | 2.4045 | C8···H13 | 3.2454 |
O1···H10 | 3.0621 | C8···H15 | 3.5497 |
O1···H10 | 3.2474 | C8···H21 | 2.9823 |
O1···H11 | 2.8446 | C11···N3 | 3.310 (3) |
O1···H21 | 3.2181 | C11···C13 | 2.434 (3) |
O1···H22 | 3.3756 | C11···C14 | 2.834 (3) |
O1···H23 | 1.8758 | C11···C15 | 2.445 (3) |
O1···H24 | 2.9984 | C11···C17 | 2.537 (3) |
O1···H25 | 3.5617 | C11···C19 | 3.580 (3) |
O1···H26 | 1.9916 | C11···H4 | 3.5879 |
O2···O4 | 2.752 (4) | C11···H5 | 2.0323 |
O2···O31 | 2.811 (8) | C11···H6 | 3.2676 |
O2···O32 | 2.473 (8) | C11···H8 | 3.2816 |
O2···O32 | 3.095 (8) | C11···H9 | 3.3395 |
O2···C18 | 3.351 (4) | C11···H13 | 2.8039 |
O2···C19 | 3.569 (4) | C11···H14 | 3.0879 |
O2···H2 | 3.5273 | C11···H15 | 2.9811 |
O2···H2 | 3.4747 | C12···C13 | 3.574 (3) |
O2···H7 | 3.2407 | C12···C14 | 2.411 (4) |
O2···H8 | 3.2947 | C12···C15 | 2.765 (3) |
O2···H10 | 3.2540 | C12···C16 | 2.424 (3) |
O2···H11 | 2.8524 | C12···C19 | 3.577 (3) |
O2···H12 | 2.9041 | C12···H1 | 3.1184 |
O2···H21 | 2.9788 | C12···H6 | 2.0053 |
O2···H22 | 1.8564 | C12···H6 | 3.1470 |
O2···H23 | 3.5104 | C12···H7 | 3.2498 |
O2···H24 | 3.5551 | C12···H13 | 2.8499 |
O2···H25 | 3.1739 | C12···H14 | 3.2193 |
O2···H27 | 1.9766 | C12···H15 | 3.3067 |
O2···H28 | 3.3621 | C13···C12 | 3.574 (3) |
O2···H29 | 3.3062 | C13···C15 | 2.389 (3) |
O2···H29 | 3.1276 | C13···C16 | 2.797 (3) |
O2···H30 | 2.2887 | C13···H1 | 3.2107 |
O2···H30 | 2.2509 | C13···H1 | 3.5160 |
O2···H31 | 3.2529 | C13···H5 | 2.0003 |
O2···H31 | 3.2804 | C13···H5 | 3.3238 |
O4···O2 | 2.752 (4) | C13···H6 | 3.5025 |
O4···O2 | 2.752 (4) | C13···H7 | 2.0356 |
O4···O31 | 3.468 (7) | C13···H8 | 3.2279 |
O4···O31 | 3.468 (7) | C13···H12 | 3.4011 |
O4···O32 | 3.201 (8) | C13···H14 | 3.2282 |
O4···O32 | 3.201 (8) | C13···H14 | 3.5974 |
O4···N1 | 2.920 (3) | C13···H15 | 3.4541 |
O4···N1 | 2.920 (3) | C14···O31 | 3.579 (7) |
O4···N6 | 3.524 (3) | C14···C2 | 3.572 (3) |
O4···N6 | 3.524 (3) | C14···C16 | 2.439 (3) |
O4···H2 | 2.9108 | C14···H1 | 3.3521 |
O4···H2 | 2.9108 | C14···H1 | 3.5629 |
O4···H24 | 1.9738 | C14···H5 | 3.2438 |
O4···H24 | 1.9738 | C14···H5 | 3.2957 |
O4···H25 | 2.6932 | C14···H6 | 2.0259 |
O4···H25 | 2.6932 | C14···H8 | 2.0024 |
O4···H26 | 3.3601 | C14···H12 | 3.1650 |
O4···H26 | 3.3601 | C14···H27 | 3.4767 |
O4···H28 | 2.9719 | C14···H28 | 3.4259 |
O4···H28 | 2.9719 | C14···H29 | 3.4074 |
O4···H29 | 3.0730 | C14···H30 | 3.5722 |
O4···H29 | 3.0730 | C15···N3 | 3.371 (3) |
O4···H30 | 2.9842 | C15···C2 | 3.440 (3) |
O4···H30 | 2.9842 | C15···C2 | 3.475 (3) |
O11···N9 | 2.818 (2) | C15···C4 | 3.539 (3) |
O11···N11 | 2.896 (2) | C15···C17 | 2.426 (3) |
O11···N12 | 3.175 (3) | C15···H1 | 3.4648 |
O11···C8 | 2.933 (3) | C15···H6 | 3.2283 |
O11···C12 | 2.329 (3) | C15···H7 | 2.0171 |
O11···C16 | 2.446 (3) | C15···H9 | 2.5330 |
O11···C17 | 3.016 (3) | C15···H29 | 3.3421 |
O11···C19 | 3.415 (3) | C15···H30 | 3.5337 |
O11···H4 | 2.4481 | C16···N3 | 3.305 (3) |
O11···H5 | 2.4854 | C16···C2 | 3.526 (3) |
O11···H13 | 2.5284 | C16···C4 | 3.597 (3) |
O11···H14 | 3.5921 | C16···C4 | 3.532 (3) |
O11···H14 | 3.5562 | C16···H5 | 3.2657 |
O11···H15 | 2.3931 | C16···H7 | 3.2780 |
O31···O32 | 1.80 (1) | C16···H8 | 2.0338 |
O31···O32 | 3.22 (1) | C16···H9 | 2.0430 |
O31···N1 | 3.260 (6) | C16···H14 | 3.3473 |
O31···N6 | 2.877 (7) | C17···O1 | 3.327 (3) |
O31···C2 | 3.361 (7) | C17···N9 | 3.340 (3) |
O31···C14 | 3.579 (7) | C17···C4 | 3.457 (3) |
O31···H1 | 2.8798 | C17···C4 | 3.508 (3) |
O31···H2 | 2.1626 | C17···C8 | 3.454 (3) |
O31···H3 | 3.1969 | C17···C18 | 2.397 (3) |
O31···H4 | 2.9093 | C17···C19 | 3.576 (3) |
O31···H5 | 2.8704 | C17···H8 | 2.5500 |
O31···H7 | 2.7626 | C17···H10 | 2.5274 |
O31···H13 | 3.2737 | C17···H11 | 2.8291 |
O31···H25 | 2.4149 | C17···H23 | 3.5427 |
O31···H26 | 3.0695 | C18···C8 | 3.482 (3) |
O31···H29 | 2.1342 | C18···C8 | 3.587 (3) |
O31···H29 | 3.2845 | C18···H4 | 3.5589 |
O31···H30 | 2.5984 | C18···H4 | 3.3141 |
O31···H30 | 3.1003 | C18···H9 | 2.4921 |
O31···H31 | 3.5264 | C18···H12 | 2.0517 |
O31···H31 | 2.8414 | C18···H13 | 2.0518 |
O32···O2 | 3.095 (8) | C18···H14 | 3.1867 |
O32···O31 | 3.22 (1) | C18···H15 | 2.6933 |
O32···N1 | 3.541 (8) | C18···H21 | 3.2942 |
O32···N1 | 2.804 (8) | C18···H22 | 3.0370 |
O32···N6 | 3.418 (7) | C18···H23 | 3.2925 |
O32···C2 | 3.491 (8) | C18···H23 | 3.5415 |
O32···C6 | 3.536 (7) | C18···H26 | 3.5256 |
O32···H1 | 3.4860 | C19···O11 | 3.415 (3) |
O32···H2 | 2.8232 | C19···C11 | 3.580 (3) |
O32···H2 | 3.3367 | C19···C12 | 3.577 (3) |
O32···H7 | 2.9837 | C19···H4 | 3.3084 |
O32···H8 | 3.2676 | C19···H5 | 3.4128 |
O32···H24 | 2.9651 | C19···H6 | 3.4534 |
O32···H24 | 3.2112 | C19···H7 | 3.4830 |
O32···H25 | 1.5928 | C19···H10 | 2.0523 |
O32···H25 | 2.2774 | C19···H11 | 2.0523 |
O32···H26 | 2.8381 | C19···H14 | 1.9783 |
O32···H26 | 3.1781 | C19···H15 | 1.9784 |
O32···H27 | 2.5445 | H1···O31 | 2.8798 |
O32···H28 | 1.5633 | H1···O32 | 3.4860 |
O32···H28 | 2.9824 | H1···C12 | 3.1184 |
O32···H29 | 2.0356 | H1···C13 | 3.2107 |
O32···H30 | 1.5218 | H1···C13 | 3.5160 |
O32···H31 | 2.9756 | H1···C14 | 3.3521 |
O32···H31 | 2.5978 | H1···C14 | 3.5629 |
N3···N1 | 2.414 (3) | H1···C15 | 3.4648 |
N3···N7 | 3.581 (3) | H2···O2 | 3.4747 |
N3···N9 | 2.450 (2) | H2···O2 | 3.5273 |
N3···N12 | 2.845 (3) | H2···O4 | 2.9108 |
N3···C6 | 2.826 (3) | H2···O31 | 2.1626 |
N3···C5 | 2.439 (3) | H2···O32 | 2.8232 |
N3···C8 | 3.482 (3) | H2···O32 | 3.3367 |
N3···C11 | 3.310 (3) | H2···N7 | 3.4287 |
N3···C15 | 3.371 (3) | H3···O1 | 3.2407 |
N3···C16 | 3.305 (3) | H3···O1 | 3.0981 |
N3···H1 | 1.9177 | H3···O31 | 3.1969 |
N3···H6 | 2.8346 | H3···N7 | 2.2382 |
N3···H8 | 3.4800 | H3···C5 | 3.4664 |
N3···H14 | 2.2204 | H3···C8 | 2.8608 |
N3···H15 | 2.8857 | H4···O31 | 2.9093 |
N1···O4 | 2.920 (3) | H4···N11 | 3.5466 |
N1···O31 | 3.260 (6) | H4···N6 | 3.2703 |
N1···O32 | 3.541 (8) | H4···C18 | 3.5589 |
N1···O32 | 2.804 (8) | H4···C18 | 3.3141 |
N1···N6 | 2.338 (3) | H4···C19 | 3.3084 |
N1···C5 | 2.367 (3) | H5···O31 | 2.8704 |
N1···C4 | 2.690 (3) | H5···C2 | 3.2989 |
N1···H1 | 1.9441 | H5···C13 | 3.3238 |
N1···H2 | 2.4871 | H5···C14 | 3.2957 |
N1···H3 | 3.1143 | H5···C19 | 3.4128 |
N1···H8 | 3.3489 | H6···N3 | 2.8346 |
N1···H24 | 3.3134 | H6···N12 | 2.8929 |
N1···H27 | 3.4487 | H6···C2 | 3.1590 |
N1···H28 | 2.3010 | H6···C12 | 3.1470 |
N1···H29 | 1.9148 | H6···C13 | 3.5025 |
N1···H30 | 3.2822 | H6···C19 | 3.4534 |
N1···H31 | 2.0022 | H7···O2 | 3.2407 |
N1···H31 | 3.4568 | H7···O31 | 2.7626 |
N7···O1 | 3.486 (3) | H7···O32 | 2.9837 |
N7···O1 | 2.960 (3) | H7···C2 | 3.5429 |
N7···N9 | 2.286 (2) | H7···C19 | 3.4830 |
N7···N6 | 3.054 (3) | H8···O1 | 3.2308 |
N7···N6 | 3.040 (3) | H8···O2 | 3.2947 |
N7···C6 | 2.544 (3) | H8···O32 | 3.2676 |
N7···C4 | 2.277 (3) | H8···N3 | 3.4800 |
N7···H2 | 3.4287 | H8···N1 | 3.3489 |
N7···H3 | 2.7951 | H8···C2 | 3.3693 |
N7···H3 | 2.2382 | H8···C6 | 3.3841 |
N7···H4 | 1.9914 | H8···C5 | 3.4608 |
N7···H9 | 3.2597 | H8···C4 | 3.4663 |
N7···H10 | 3.3034 | H9···O1 | 2.4045 |
N7···H11 | 2.8861 | H9···N7 | 3.2597 |
N7···H21 | 3.2102 | H9···N9 | 3.4503 |
N7···H21 | 2.0370 | H9···C5 | 3.3029 |
N7···H22 | 3.2549 | H9···C4 | 3.4370 |
N7···H23 | 3.1246 | H9···C8 | 3.2974 |
N9···Pd1 | 3.542 (2) | H10···O1 | 3.2474 |
N9···N11 | 3.384 (3) | H10···N7 | 3.3034 |
N9···N11 | 3.565 (3) | H10···N6 | 2.9920 |
N9···N12 | 3.001 (2) | H10···C8 | 3.0302 |
N9···C2 | 3.551 (3) | H11···N7 | 2.8861 |
N9···C6 | 3.544 (3) | H11···N9 | 3.2626 |
N9···C5 | 2.231 (3) | H11···C5 | 3.5320 |
N9···C17 | 3.340 (3) | H11···C8 | 2.6730 |
N9···H4 | 2.0139 | H12···C13 | 3.4011 |
N9···H9 | 3.4503 | H12···C14 | 3.1650 |
N9···H11 | 3.2626 | H13···O11 | 2.5284 |
N9···H14 | 2.8800 | H13···O31 | 3.2737 |
N9···H15 | 3.3139 | H13···C8 | 3.2454 |
N11···N9 | 3.384 (3) | H13···C11 | 2.8039 |
N11···N9 | 3.565 (3) | H13···C12 | 2.8499 |
N11···N12 | 2.645 (3) | H14···O11 | 3.5921 |
N11···C4 | 3.570 (3) | H14···O11 | 3.5562 |
N11···C8 | 3.535 (3) | H14···C11 | 3.0879 |
N11···C11 | 3.001 (3) | H14···C12 | 3.2193 |
N11···C16 | 2.429 (3) | H14···C13 | 3.2282 |
N11···C19 | 2.409 (3) | H14···C13 | 3.5974 |
N11···H4 | 3.5466 | H14···C16 | 3.3473 |
N11···H9 | 1.9021 | H15···Pd1 | 3.4825 |
N11···H10 | 2.0297 | H15···O11 | 2.3931 |
N11···H11 | 2.0297 | H15···C8 | 3.5497 |
N11···H12 | 3.2466 | H15···C11 | 2.9811 |
N11···H13 | 2.7112 | H15···C12 | 3.3067 |
N11···H14 | 3.4003 | H15···C13 | 3.4541 |
N11···H15 | 3.0529 | H21···O1 | 3.2181 |
N12···O11 | 3.175 (3) | H21···N7 | 3.2102 |
N12···C4 | 3.255 (3) | H21···N7 | 2.0370 |
N12···C18 | 2.412 (3) | H21···N6 | 2.9904 |
N12···H6 | 2.8929 | H21···N6 | 3.2328 |
N12···H10 | 3.2494 | H21···C6 | 3.4682 |
N12···H11 | 2.7146 | H21···C6 | 3.3721 |
N12···H12 | 2.0300 | H21···C5 | 3.4947 |
N12···H13 | 2.0299 | H21···C5 | 2.8383 |
N6···O1 | 3.529 (3) | H21···C8 | 2.9823 |
N6···O4 | 3.524 (3) | H22···O1 | 3.3756 |
N6···O31 | 2.877 (7) | H22···N7 | 3.2549 |
N6···O32 | 3.418 (7) | H22···N6 | 3.4600 |
N6···N7 | 3.040 (3) | H22···N6 | 3.4645 |
N6···C2 | 3.561 (3) | H23···O1 | 1.8758 |
N6···C5 | 2.416 (3) | H23···N7 | 3.1246 |
N6···C8 | 3.535 (3) | H23···N6 | 3.3156 |
N6···H4 | 3.2703 | H23···C6 | 3.5793 |
N6···H10 | 2.9920 | H23···C5 | 3.4419 |
N6···H21 | 2.9904 | H23···C17 | 3.5427 |
N6···H21 | 3.2328 | H23···C18 | 3.5415 |
N6···H22 | 3.4645 | H24···O2 | 3.5551 |
N6···H22 | 3.4600 | H24···O4 | 1.9738 |
N6···H23 | 3.3156 | H24···O32 | 3.2112 |
N6···H24 | 3.2448 | H24···N1 | 3.3134 |
N6···H26 | 3.0756 | H24···N6 | 3.2448 |
N6···H27 | 2.9414 | H24···C6 | 3.5044 |
N6···H28 | 3.4332 | H25···O2 | 3.1739 |
N6···H29 | 2.9958 | H25···O4 | 2.6932 |
N6···H31 | 3.0911 | H25···O32 | 2.2774 |
C2···O31 | 3.361 (7) | H26···O4 | 3.3601 |
C2···O32 | 3.491 (8) | H26···O32 | 3.1781 |
C2···C6 | 2.322 (3) | H26···N6 | 3.0756 |
C2···C5 | 2.655 (3) | H26···C6 | 3.3969 |
C2···C4 | 2.223 (3) | H27···O32 | 2.5445 |
C2···C14 | 3.572 (3) | H27···N1 | 3.4487 |
C2···C15 | 3.440 (3) | H27···N6 | 2.9414 |
C2···C15 | 3.475 (3) | H27···C14 | 3.4767 |
C2···C16 | 3.526 (3) | H28···O32 | 2.9824 |
C2···H5 | 3.2989 | H28···N1 | 2.3010 |
C2···H6 | 3.1590 | H28···N6 | 3.4332 |
C2···H7 | 3.5429 | H28···C2 | 2.5028 |
C2···H8 | 3.3693 | H28···C6 | 3.4970 |
C2···H14 | 3.3617 | H28···C14 | 3.4259 |
C2···H28 | 2.5028 | H29···O2 | 3.1276 |
C2···H29 | 2.6646 | H29···O31 | 3.2845 |
C2···H31 | 2.9218 | H29···O32 | 2.0356 |
C6···O32 | 3.536 (7) | H29···N1 | 1.9148 |
C6···C4 | 2.392 (3) | H29···N6 | 2.9958 |
C6···C8 | 3.508 (3) | H29···C2 | 2.6646 |
C6···H1 | 3.1395 | H29···C6 | 2.6299 |
C6···H2 | 1.9327 | H29···C14 | 3.4074 |
C6···H3 | 1.9326 | H29···C15 | 3.3421 |
C6···H8 | 3.3841 | H30···O2 | 2.2509 |
C6···H21 | 3.4682 | H30···O4 | 2.9842 |
C6···H21 | 3.3721 | H30···O31 | 3.1003 |
C6···H23 | 3.5793 | H30···O32 | 1.5218 |
C6···H24 | 3.5044 | H30···N1 | 3.2822 |
C6···H26 | 3.3969 | H30···C14 | 3.5722 |
C6···H28 | 3.4970 | H30···C15 | 3.5337 |
C6···H29 | 2.6299 | H31···O2 | 3.2529 |
C6···H31 | 2.9174 | H31···O2 | 3.2804 |
C5···C8 | 2.117 (3) | H31···O31 | 2.8414 |
C5···H1 | 3.5849 | H31···O32 | 2.5978 |
C5···H2 | 3.1863 | H31···N1 | 2.0022 |
C5···H3 | 2.5729 | H31···N1 | 3.4568 |
C5···H3 | 3.4664 | H31···N6 | 3.0911 |
C5···H4 | 3.0142 | H31···C2 | 2.9218 |
C5···H8 | 3.4608 | H31···C6 | 2.9174 |
C5···H9 | 3.3029 | ||
O11—Pd1—N9 | 88.73 (7) | H1—C2—N3 | 115.5634 |
O11—Pd1—N11 | 93.97 (7) | H1—C2—N1 | 115.5581 |
O11—Pd1—N12 | 175.05 (7) | C5—C6—N1 | 118.2 (2) |
N9—Pd1—N11 | 175.49 (7) | C5—C6—N6 | 122.4 (2) |
N9—Pd1—N12 | 94.88 (7) | C4—C5—N7 | 110.4 (2) |
N11—Pd1—N12 | 82.65 (8) | C4—C5—C6 | 117.6 (2) |
H21—O1—H22 | 97.6848 | H4—C8—N9 | 122.0074 |
H21—O1—H23 | 97.4770 | H4—C8—N7 | 122.0222 |
H22—O1—H23 | 126.3031 | C12—C11—O11 | 116.7 (2) |
H24—O2—H25 | 94.5744 | C12—C11—C16 | 117.6 (2) |
H24—O2—H26 | 94.7639 | C16—C11—O11 | 125.7 (2) |
H25—O2—H26 | 111.2363 | C13—C12—C11 | 121.8 (2) |
H31—O4—H31 | 112.1156 | C13—C12—H5 | 119.0932 |
C11—O11—Pd1 | 123.9 (1) | H5—C12—C11 | 119.0956 |
H27—O31—H28 | 94.0121 | C14—C13—C12 | 120.8 (2) |
O32—O32—H27 | 135.3002 | C14—C13—H6 | 119.6213 |
O32—O32—H29 | 103.9991 | H6—C13—C12 | 119.6133 |
O32—O32—H30 | 68.6305 | C15—C14—C13 | 118.8 (2) |
H27—O32—H29 | 119.5179 | C15—C14—H7 | 120.5932 |
H27—O32—H30 | 114.0558 | H7—C14—C13 | 120.6134 |
H29—O32—H30 | 95.0762 | C16—C15—C14 | 121.9 (2) |
C2—N3—C4 | 112.1 (2) | C16—C15—H8 | 119.0715 |
C2—N1—C6 | 118.1 (2) | H8—C15—C14 | 119.0747 |
C5—N7—C8 | 102.4 (2) | C17—C16—C11 | 124.5 (2) |
C4—N9—Pd1 | 130.5 (1) | C17—C16—C15 | 116.3 (2) |
C4—N9—C8 | 103.8 (2) | H9—C17—N11 | 117.2095 |
C8—N9—Pd1 | 125.6 (1) | H9—C17—C16 | 117.2190 |
C17—N11—Pd1 | 125.9 (1) | C19—C18—N11 | 107.6 (2) |
C17—N11—C18 | 119.9 (2) | C19—C18—H11 | 110.1830 |
C18—N11—Pd1 | 114.3 (1) | C19—C18—H10 | 110.1829 |
C19—N12—Pd1 | 108.3 (1) | H10—C18—N11 | 110.1800 |
C19—N12—H14 | 110.0450 | H10—C18—H11 | 108.4805 |
C19—N12—H15 | 110.0486 | H11—C18—N11 | 110.1761 |
H14—N12—Pd1 | 110.0440 | H12—C19—N12 | 110.1575 |
H14—N12—H15 | 108.3900 | H12—C19—C18 | 110.1268 |
H15—N12—Pd1 | 110.0544 | H12—C19—H13 | 108.4661 |
C6—N6—H2 | 120.0043 | H13—C19—N12 | 110.1493 |
C6—N6—H3 | 120.0181 | H13—C19—C18 | 110.1372 |
H2—N6—H3 | 119.9776 | ||
N9—Pd1—O11—C11 | 169.3 (2) | Pd1—N12—C19—C18 | −43.9 (2) |
O11—Pd1—N9—C4 | 175.4 (2) | H2—N6—C6—N1 | 0.0 |
O11—Pd1—N11—C17 | 6.3 (2) | N1—C6—C5—N7 | 179.7 (2) |
Pd1—O11—C11—C12 | −175.0 (2) | N6—C6—C5—N7 | −0.1 (3) |
H28—O31—H27—O32 | 18.2 | N7—C5—C4—N3 | −179.7 (2) |
H29—O32—H27—O31 | −41.5 | N7—C5—C4—N9 | 0.4 (2) |
C4—N3—C2—N1 | −1.5 (3) | C6—C5—C4—N3 | 1.4 (3) |
C2—N3—C4—N9 | 180.0 (2) | C6—C5—C4—N9 | −178.5 (2) |
C2—N3—C4—C5 | 0.1 (2) | O11—C11—C12—C13 | −179.3 (2) |
C6—N1—C2—N3 | 1.2 (4) | O11—C11—C16—C15 | 178.7 (2) |
C2—N1—C6—N6 | −179.6 (2) | C11—C12—C13—C14 | 0.3 (4) |
C8—N7—C5—C6 | 178.2 (2) | C12—C13—C14—C15 | −0.6 (4) |
C5—N7—C8—N9 | 0.4 (2) | C13—C14—C15—C16 | 0.0 (3) |
Pd1—N9—C4—N3 | −4.7 (3) | C14—C15—C16—C11 | 0.8 (3) |
Pd1—N9—C4—C5 | 175.2 (2) | C11—C16—C17—N11 | −1.4 (3) |
Pd1—N9—C8—N7 | −175.9 (2) | C15—C16—C17—N11 | −179.9 (2) |
Pd1—N11—C17—C16 | −3.3 (3) | N11—C18—C19—N12 | 46.0 (2) |
Pd1—N11—C18—C19 | −27.3 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
N12—H14···N3 | 0.90 | 2.22 | 2.845 (4) | 126 |
N12—H15···O11i | 0.90 | 2.39 | 3.175 (3) | 145 |
N6—H3···N7ii | 0.86 | 2.24 | 3.040 (3) | 155 |
O4—H31···N1iii | 0.99 | 2.00 | 2.920 (3) | 154 |
O4—H31iv···N1v | 0.99 | 2.00 | 2.920 (3) | 154 |
O1—H21···N7i | 0.93 | 2.04 | 2.960 (3) | 170 |
O1—H22···O2 | 0.94 | 1.86 | 2.783 (4) | 167 |
O2—H24···O4vi | 0.95 | 1.97 | 2.752 (4) | 137 |
O2—H25···O32 | 0.96 | 1.59 | 2.473 (8) | 151 |
O32—H29···N1v | 0.96 | 1.92 | 2.804 (6) | 154 |
O32—H30···O2iv | 0.96 | 2.25 | 3.095 (8) | 146 |
O1—H23···O1vii | 0.95 | 1.88 | 2.793 (4) | 163 |
O2—H26···O1 | 0.95 | 1.99 | 2.783 (4) | 139 |
O31—H27···O2 | 0.96 | 1.98 | 2.811 (8) | 144 |
O31—H28···N1v | 0.96 | 2.30 | 3.260 (7) | 179 |
N6iii—H2iii···O31 | 0.86 | 2.16 | 2.877 (6) | 140 |
Symmetry codes: (i) −x+1/2, −y+3/2, −z; (ii) −x, −y+2, −z; (iii) x+1/2, y−1/2, z; (iv) −x+1, y, −z+1/2; (v) −x+1/2, y−1/2, −z+1/2; (vi) x, y+1, z; (vii) −x+1, −y+2, −z. |